Candidates for 2016 ERP of the Year

46 / 328

SPIFAN Expert Review Panel Report
September 29, 2015
Final Version
Page 2
I. WELCOME AND INTRODUCTIONS
Darryl Sullivan welcomed all participants to the ERP meeting and introduced the ERP members.
II. REVIEW OF METHODS BY EXPERT REVIEW PANEL (ERP) FOR FIRST ACTION OFFICIAL METHODSM
STATUS – AOAC SPIFAN I
For each method, the ERP/Working Group Chairs including (Co-Chairs) discussed methods submitted.
Method Method Title Reviewer(s) Vote Comments
Carnitine/
Choline
Carn-06 - Carnitine
Quantitated by liquid
chromatography and isotope
dilution and Choline
quantitated by liquid
chromatography and isotope
dilution mass spectroscopy
Sneh Bhandari
John Austad
Method not adopted/
moved to First Action
Official MethodSM status
 Method can analyze for free and total Carnitine
 Validation data includes different units
 Spiked recovery in the data but not in the
evaluation form
 1849a used to establish free Carnitine
 The method is well designed and employs internal
standard for precision purposes
 The method is MS based and thus quite specific
to the analyte it measures.
 Method Author to provide ERP with information
on retention time
III. REVIEW OF METHODS BY EXPERT REVIEW PANEL (ERP) FOR FIRST ACTION OFFICIAL METHODSM
STATUS – AOAC SPIFAN II
For each method, the ERP/Working Group Co-Chairs discussed methods submitted. Nine (9) methods were received
and reviewed and one (1) method received First Action Official MethodSM status.
Method Method Title Reviewer(s) Vote Comments
Amino Acid Amino-02 - HPLC
Determination of Total
Tryptophan in Infant Formula
and Adult/Pediatric
Nutritional Formula Following
Enzymatic Hydrolysis
Maria Ofitserova
Shay Phillips
Method not adopted/
moved to First Action
Official MethodSM status
 The amino acid profile only measures tryptophan
 For chosen samples the method showed good
precision and accuracy.
 Data for NIST SRM 1849a is presented for 2
laboratories and accuracy for this matrix meets
SMPR.
 The sample prep takes less time
 Sample size is too small/precision
 No SPIFAN matrices were used for validation.
Limited data for 3 matrices are presented – NIST
SRM 1849a, soy formula and Hypoallergenic
formula.
o Method needs more data on SPIFAN materials
 Method uses 3-point calibration instead of
recommended 6-point and no information on the
range is given.
 Actual levels of Tryptophan in studied matrices
(except for NIST SRM 1849a) and spike levels used
for accuracy studies are not listed.
 Background Tryptophan from self-digest of
enzymes in the absence of the sample is a concern
since this can affect accuracy of analysis at low
levels.
 One weakness is the limit of quantitation range
 Provide additional information on the following:
o Analytical range
o wide calibration range
o system suitability
Carotenoids Carot-01 - Determination of
Carotenoids in Infant Formula
and Adult/Pediatric
Nutritional Formula using
High-Performance Liquid
Chromatography with Photo
Diode Array Detection.
Jon DeVries
Adrienne
McMahon
Method not adopted/
moved to First Action
Official MethodSM status
 Method uses best of the technology available for
Carotenoids
 Use of internal standards & PKB columns could
improve
 Need safety comments for the isopropyl ether/
peroxides
 determination of the beta carotene stock solution
needs a second step
 Mobil phase D has to be stirred constantly
 A working standard injection is specified, but
nothing on how to prepare or any chromatograms
o Information provided on six (6) samples and one
(1) lab
o Awaiting additional data
 Good method, but needs additional work and
clarification on standards (include control sample)
and purity checks
 Need to see a standard chromatogram (including
reference)
 Method needs enough samples of Carotenoids to
do an SLV
 Temperature is very high (85˚)
ERP PROFILE SUMMARIES
45